Small-scale reactor for data oriented process development

During the early stages of research and development chemical industry needs flexible and versatile tools to investigate chemical reaction systems. An important part of the optimisation of a process considering economic factors, risk analysis and environmental impacts is the determination of a reaction mechanism and its associated parameters (i.e. activation energies, rates and heat of reactions). <br><br> We present here a new fully automated small-scale reaction calorimeter combining a power-compensation heater and a thermoelectrically regulated metal surrounding. This dual temperature control makes the reactor highly suitable for fast and exothermic reactions and eliminates the need for time-consuming calibration of heat transfer coefficients. With a working volume from 25 to 45ml the device is particularly suited for the fine and pharmaceutical chemical industries where only small amounts of test substances are available. <br><br> An integrated ATR-IR probe coupled to an FT-IR spectrometer allows the investigation of complex reaction mechanisms. Moreover, the new reactor design allows the simultaneous use of various additional in-situ analytics such as UV-Vis, gas intake/uptake and particle size analysis. The performance of the new reaction calorimeter has already been successfully demonstrated based on several reactions [1, 2, 3]. <br><br> Different analytical techniques may point to different optimum reaction parameters. Algorithms and mathematical tools, such as multi-objective multivariate kinetic modelling, become an important research area in data oriented process development. Only a short introduction into these methods will be given here. <br><br> [1] Zogg, A., Fischer, U., & Hungerbühler, K. (2003). A new small-scale reaction calorimeter that combines the principles of power compensation and heat balance. Industrial & Engineering Chemistry Research, 42, 767-776. <br> [2] Visentin, F., Gianoli, S. I., Zogg, A., Kut, O. M., & Hungerbühler, K. (2004). Pressure-resistant smallscale reaction calorimeter that combines the principles of power compensation and heat balance (CRC.v4). Organic Process Research & Development, 8(5), 725-737. <br> [3] Visentin, F., Puxty, G., Kut, O. M., & Hungerbühler, K. (2006). Study of the hydrogenation of selected nitro compounds by simultaneous measurements of calorimetric, FT-IR, and gas-uptake signals. Industrial & Engineering Chemistry Research, 45(13), 4544-4553.

Presented at:

Symposium of the Swiss Society for Thermal Analysis and Calorimetry (STK), Lausanne (Switzerland), June 14, 2007